CN103353451B - Preparation method of nano probe - Google Patents
Preparation method of nano probe Download PDFInfo
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- CN103353451B CN103353451B CN201310278173.5A CN201310278173A CN103353451B CN 103353451 B CN103353451 B CN 103353451B CN 201310278173 A CN201310278173 A CN 201310278173A CN 103353451 B CN103353451 B CN 103353451B
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Abstract
The invention provides a preparation method of a nano probe. The method comprises the steps as follows: (1) performing surface cleaning treatment to a silicone-based or carborundum-based probe, and arranging a cover on the whole probe except the point; (2) coating the silicone-based or carborundum-based probe with a nano-granularity noble metal film, noble metal alloy film or noble metal lamination through a vacuum evaporation coating technology or a magnetron sputtering technology, and removing the cover; (3) carrying out a TERS (Tip enhanced Raman spectroscopy) experiment on a nano probe prepared on TERS equipment, and counting the corresponding relations between enhanced properties of the nano probe and technical parameters of preparation according to experimental results; (4) adjusting the technical parameters of preparation according to the corresponding relations, and repeating the steps (1) to (4) until the nano probe meeting preset enhancement conditions is obtained.
Description
Technical field
The application relates to field of nanometer devices, particularly relates to a kind of preparation method of nano-probe.
Background technology
Raman spectrum and Surface enhanced raman spectroscopy, as a kind of analytical technology means, can obtain the relevant information on intramolecule vibration, absorption behavior and material structure and surface thereof.But by the restriction of optical diffraction limit, the spatial resolution of conventional far-field Raman spectrum cannot break through the restriction of optical diffraction half-wavelength, the average information of plurality of samples chemical composition in certain area can only be obtained, the spectral information of nano-space resolution and local pattern can not be obtained simultaneously.Based on the TERS(Tip enhanced Ramanspectroscopy of near field optic principle and scanning probe microscopy (SPM), Tip-Enhanced Raman Spectroscopy) appearance of technology solves this Raman spectroscopy problem.
But, since TERS technology is in the news, TERS technology progress experimentally more than people envision slow.The development of TERS technology and design level and the structural behaviour of application except depending on optically coupled system, the research and development technology level of TERS nano-probe also plays very important effect to the development of TERS technology simultaneously.Thus, the TERS nano-probe meeting TERS technical need how is provided to be a problem demanding prompt solution.
Summary of the invention
The object of this invention is to provide a kind of preparation method of nano-probe, can provide and there is the excellent TERS nano-probe strengthening effect.
For achieving the above object, the invention provides a kind of preparation method of nano-probe, comprising:
Step (1), carries out surface cleaning process to silica-based or silicon carbide-based probe, and blocks in the part setting except needle point;
Step (2), at described silica-based or silicon carbide-based detecting probe surface by vacuum evaporation coating membrane technology evaporation or by the magnetron sputtering technique sputtering noble metal film of nano particle size, precious metal alloys film or noble metal lamination, and blocks described in removing;
Step (3), needle point strengthens and Raman spectrum TERS equipment applies obtained nano-probe carries out TERS experiment, and experimentally result adds up the corresponding relation of the enhanced propertied of described nano-probe and preparation technology parameter;
Step (4), adjusts described preparation technology parameter according to described corresponding relation, repeats step (1)-(3), until be met the nano-probe of default enhancing condition.
Wherein, block can comprise in the part setting except needle point: at the Wax-coated layer of described part except needle point or stickup barrier bed.
Wherein, described by vacuum evaporation coating membrane technology evaporation or by magnetron sputtering technique sputtering nano particle size precious metal alloys film can comprise:
The gold and silver target that molar ratio is 1:1 to 1:3 is set, uses described gold and silver target that described precious metal alloys film is set.
Wherein, the described precious metal alloys film by vacuum evaporation coating membrane technology evaporation nano particle size can comprise: heat described silica-based or silicon carbide-based probe.
Wherein, described by vacuum evaporation coating membrane technology evaporation or by magnetron sputtering technique sputtering nano particle size noble metal lamination can comprise:
Two or more noble metal target material is set simultaneously, is used alternatingly described two or more noble metal target material and carries out evaporation or sputtering obtains noble metal lamination.
Wherein, described two or more noble metal target material can comprise gold and silver-colored target, carries out evaporation or sputtering obtains Yin-Jin-Yin lamination according to order that is silver-colored, gold, silver target.
Can also comprise before step (2):
Between described silica-based or silicon carbide-based probe and noble metal target material, precious metal network is set, the closer to needle point position described in the density of mesh of precious metal network less.
Wherein, described precious metal network can comprise the structure of the proportional amplification of needle point of described silica-based or silicon carbide-based probe, and the needle point of described silica-based or silicon carbide-based probe is contained in described precious metal network.
Can also comprise before step (2): heat described silica-based or silicon carbide-based probe.
Based on technique scheme, the present invention, by arranging nanometer layer at silica-based or silicon carbide-based detecting probe surface, obtains nano-probe.Because silica-based or silicon carbide-based probe has stronger hardness, therefore, the nano-probe obtained by the present invention has stronger hardness, can be applied more broadly in spectral detection.And, owing to testing with TERS the adjusting process parameter that combines, the noble metal nano layer having and better strengthen effect can be obtained.
Accompanying drawing explanation
Accompanying drawing described herein is used to provide a further understanding of the present invention, and form a application's part, schematic description and description of the present invention, for explaining the present invention, does not form inappropriate limitation of the present invention.In the accompanying drawings:
The schematic flow sheet of the preparation method of the nano-probe that Fig. 1 provides for the application.
The schematic diagram of the process of silver nanoparticle film prepared by the silicon probe that Fig. 2 provides for the embodiment of the present application one.
The schematic diagram of the process of silver nanoparticle film prepared by the silicon probe that Fig. 3 provides for the embodiment of the present application two.
The schematic diagram of the process of silver nanoparticle film prepared by the silicon probe that Fig. 4 provides for the embodiment of the present application three.
Embodiment
Below by drawings and Examples, technical scheme of the present invention is described in further detail.
The application provides a kind of preparation method of nano-probe, as shown in Figure 1, comprising:
Step 101, carries out surface cleaning process to silica-based or silicon carbide-based probe, and blocks in the part setting except needle point.
May be there is greasy dirt or other impurity in silica-based or silicon carbide-based detecting probe surface, need first to carry out surface cleaning process, removes these greasy dirts or other impurity.The mode of surface cleaning process comprises to be made chemically or physical method cleans, such as, with an organic solvent wash silica-based or silicon carbide-based detecting probe surface, or, use the silica-based or silicon carbide-based detecting probe surface of sand papering etc.Preferably, five step ultrasonic cleaning methods are used to carry out cleaning to silica-based or silicon carbide-based detecting probe surface in the application, concrete steps comprise: use deionized water-absolute ethyl alcohol-acetone-absolute ethyl alcohol-deionized water to nano-probe ultrasonic cleaning five minutes in turn respectively, then carry out vacuum drying treatment to the needle point after cleaning.
In present embodiment, for silica-based or silicon carbide-based detecting probe surface, only layer of precious metal is set at needle point position, thus avoids the nanostructured noble metal in TERS experiment outside needle point to have influence on overall enhancing effect.Therefore, need the part in advance outside needle point to arrange block thus avoid part outside the needle point of silica-based or silicon carbide-based probe to arrange nano particle size noble metal.The concrete mode of blocking includes but not limited to Wax-coated layer, tygon organic coating, or pastes other barrier bed, and these shielding modes need be easy to be eliminated follow-up and can not bring other impurity on probe.
Step 102, at silica-based or silicon carbide-based detecting probe surface by vacuum evaporation coating membrane technology evaporation or by the magnetron sputtering technique sputtering noble metal film of nano particle size, precious metal alloys film or noble metal lamination, and with an organic solvent removes and blocks.
Arrange nano-noble metal layer by vacuum evaporation coating membrane technology evaporation or by magnetron sputtering technique in the application, concrete setting procedure will be introduced in detail in Examples below.After coating is set, also need to remove the coating outside needle point, now block owing to being provided with in step 101, therefore, remove while blocking and just can remove the coating blocked, the probe stayed only is provided with nano-noble metal coating at needle point position, and the organic solvent wherein used comprises absolute ethyl alcohol, acetone etc.
Step 103, TERS equipment is applied obtained nano-probe and carries out TERS experiment, experimentally the corresponding relation of the enhanced propertied and preparation technology parameter of result statistics nano-probe.
In order to ensure the consistance that TERS tests, in the application, once obtained tested reagent is divided into many parts, each TERS experiment uses a copy of it reagent, thus ensures to greatest extent to cause TERS to strengthen the change of effect by the change of nano-probe.Preparation technology parameter specifically includes but not limited to sputtering time, argon flow amount, underlayer temperature, sputtering voltage-electric current and target lining spacing etc.
Step 104, according to above-mentioned corresponding relation adjustment preparation technology parameter, repeats step 101 to 104, until be met the nano-probe of default enhancing condition.
Preset enhancing condition for the enhancing rank preset, to be determined according to actual needs by user, be not restricted this herein.
In the application, consider the difference of vacuum thermal evaporation coating technique and magnetron sputtering technique, preferably, wrap up one deck precious metals as gold or silver nanoparticle film by the means of vacuum thermal evaporation plated film at such as existing silica-based needle surface, the preparation TERS formula of rapping (DFM) strengthens nanometer pinpoint; Adopt magnetron sputtering means at existing silicon carbide-based contact (AFM) needle surface trapping gold/silver alloy nano thin-film or Yin-Jin-Yin Sanming tobacco-growing areas, strengthen TERS AFM for the preparation of microcell scanning and strengthen nanometer pinpoint.Further, the TERS equipment pre-set is applied prepared all kinds of nanometers and strengthen probe, the enhancing efficiency of full test probe and the relation of preparation technology parameter, and then the adjustment state modulator needle point pattern of system; The parameter index such as thickness, roughness of needle surface coating noble metal nano thin-film, reaches desirable TERS and strengthens effect.
The preparation method of the nano-probe that the application provides is illustrated below by embodiment.
Embodiment one
The present embodiment provides a kind of preparation method of nanometer pinpoint, be introduced to prepare silver nanoparticle film at silicon detecting probe surface, be to be understood that, use silicon carbide-based probe, or use other precious metals situation as described in the situation of gold, platinum etc. and the present embodiment similar, can carry out with reference to process described in the present embodiment, i.e. the present embodiment be not used in and the preparation of nano-probe be restricted to certain probe concrete or certain noble metal.
The process of silver nanoparticle film is prepared in lower mask body introduction on silicon probe, as shown in Figure 2, comprises the following steps:
Step 201, carries out surface cleaning process to silicon probe.
This step and step 101 are similar, can refer step 101, do not repeat them here.
Step 202, wraps up one deck silver nanoparticle film by the technology of vacuum thermal evaporation plated film at silicon detecting probe surface, preparation TERS silver nanoparticle needle point.
For promoting carrying out smoothly of plated film, except controlling the temperature of silver-colored target, can also heat silicon needle point.
In addition, in order to control the homogeneity of silverskin on silver nanoparticle needle point, can arrange silver-colored net between silicon needle point and silver-colored target, the density of the mesh of silver net is lower the closer to needle point.In this way, intervene target molecule in vacuum chamber and, to the distribution probability of detecting probe surface, improve the homogeneity on argentum nanometer probe surface.
The concrete shape of silver net can be arranged flexibly according to actual conditions, the overall proportional increase of silicon probe relatively of silver net such as can be set, namely silver-colored net global shape is also probe shape, and silicon probe is contained in silver net, and the Argent grain that silver-colored target is evaporated arrives silicon probe by the mesh of silver net.
Step 203, TERS equipment is applied obtained nano-probe and carries out TERS experiment, experimentally the corresponding relation of the enhanced propertied and preparation technology parameter of result statistics nano-probe.
Technological parameter includes but not limited to the evaporating temperature of silver-colored target, vacuum tightness and target lining spacing etc.
Other operations of this step can refer step 103, repeats no more herein.
Step 204, according to above-mentioned corresponding relation adjustment preparation technology parameter, repeats step 201 to 204, until be met the nano-probe of default enhancing condition.
In this step, according to the material i.e. material boiling point of silver and the saturated vapor pressure of institute's evaporation, determine best evaporating temperature and vacuum tightness, such that the thickness of the Ag films of silicon needle surface is moderate, dense, smooth surface, the good difficult drop-off of absorption property of film and tip point material.In the present embodiment, control evaporation rate by controlling evaporation molybdenum boat electric current, in the application, the evaporation molybdenum boat electric current of silver-colored target is at 100-120 ampere, preferably 115 amperes.
Embodiment two
The present embodiment provides a kind of preparation method of nanometer pinpoint, is introduced to prepare electrum nano thin-film at silit detecting probe surface.Similar with embodiment one, be to be understood that, use silicon probe, or use other precious metals situation as described in the situation of plation, silver-platinum alloy etc. and the present embodiment similar, the present embodiment is also not used in the preparation of nano-probe is restricted to specifically certain probe or certain noble metal.
The process of electrum nano thin-film is prepared in lower mask body introduction on silit probe, as shown in Figure 3, comprises the following steps:
Step 301, carries out surface cleaning process to silicon probe.
This step and step 101 are similar, can refer step 101, do not repeat them here.
Step 302, sputters one deck electrum nano thin-film with magnetron sputtering technique at silit detecting probe surface, preparation TERS electrum nanometer pinpoint.
For promoting carrying out smoothly of plated film, can heat silit needle point.
With in a upper embodiment similarly, in order to control the homogeneity of electrum on nanometer silicon carbide needle point, between silit needle point and gold and silver target, correspondingly can arrange golden net or silver-colored net or electrum net, the density of mesh is lower the closer to needle point.
In order to prepare the electrum nano thin-film of applicable TERS, the content of wherein gold and silver can be adjusted.Such as, the content of gold and silver in electrum film is adjusted by the gold target material of adjustment use and the content of silver-colored target.
Step 303, TERS equipment is applied obtained electrum nano-probe and carries out TERS experiment, experimentally the corresponding relation of the enhanced propertied and preparation technology parameter of result statistics gold and silver nano-probe.
Technological parameter includes but not limited to sputtering rate, the vacuum tightness of gold and silver target and target serves as a contrast spacing, the content of gold and silver compares.
Other operations of this step can refer step 103, repeats no more herein.
Step 304, according to above-mentioned corresponding relation adjustment preparation technology parameter, repeats step 301 to 304, until be met the nano-probe of default enhancing condition.
In this step, adjustment gold and silver content ratio, determines best gold and silver content ratio, such that the thickness of the electrum film of silicon needle surface is moderate, dense, smooth surface, the good difficult drop-off of absorption property of film and tip point material.In the present embodiment, the molar ratio of gold and silver is preferably in the scope of 1:1 to 1:3.
Embodiment three
The present embodiment provides a kind of preparation method of nanometer pinpoint, is introduced for the sandwich structure preparing Nano Silver-Jin-Yin at silit detecting probe surface.Similar with embodiment one, be to be understood that, use silicon probe, or use other precious metals situation as described in the situation of Jin-Yin-Jin, Jin-Yin-platinum etc. or more laminations and the present embodiment similar, the present embodiment is also not used in the structure preparation of nano-probe being restricted to certain probe concrete or certain noble metal or the specific number of plies.
The stacked process of Yin Jinyin Nanoalloy is prepared in lower mask body introduction on silit probe, as shown in Figure 4, comprises the following steps:
Step 401, carries out surface cleaning process to silicon probe.
This step and step 101 are similar, can refer step 101, do not repeat them here.
Step 402, with magnetron sputtering technique at silit detecting probe surface successively sputtering silver nano thin-film, gold nanometer film and silver nanoparticle film, preparation TERS Yin-Jin-Yin sandwich nanometer pinpoint.
Similar to the above embodimentsly, be promote the carrying out smoothly of plated film, can heat silit needle point, and golden net or silver-colored net or electrum net correspondingly can be set between silit needle point and gold and silver target.
In the present embodiment, two gold and silver-colored target are set simultaneously, carry out sputtering according to the order of silver, gold, silver target and obtain Yin-Jin-Yin lamination.Or, two silver medal one gold target materials are set simultaneously, carry out sputtering according to the order of silver, gold, silver target and obtain Yin-Jin-Yin lamination, thus control the thickness of every one deck better.
Step 403, TERS equipment is applied the obtained stacked probe of Yin-Jin-silver nanoparticle and carries out TERS experiment, experimentally the corresponding relation of the enhanced propertied and preparation technology parameter of the stacked probe of result statistics Yin-Jin-silver nanoparticle.
Technological parameter includes but not limited to the thickness (sputtering time) of the sputtering rate of gold and silver target, vacuum tightness and target lining spacing, each individual layer and total thickness etc.
Other operations of this step can refer step 103, repeats no more herein.
Step 404, according to above-mentioned corresponding relation adjustment preparation technology parameter, repeats step 401 to 404, until be met the nano-probe of default enhancing condition.
Although be described with sandwich structure in the present embodiment, it should be noted that and can to increase in preparation process or to reduce the number of plies, such as only prepare 2 layers or preparation more than 4 layers structures, the application is not restricted this.
Finally should be noted that: above embodiment is only in order to illustrate that technical scheme of the present invention is not intended to limit; Although with reference to preferred embodiment to invention has been detailed description, those of ordinary skill in the field are to be understood that: still can modify to the specific embodiment of the present invention or carry out equivalent replacement to portion of techniques feature; And not departing from the spirit of technical solution of the present invention, it all should be encompassed in the middle of the technical scheme scope of request of the present invention protection.
Claims (9)
1. a preparation method for nano-probe, is characterized in that, comprising:
Step (1), carries out surface cleaning process to silica-based or silicon carbide-based probe, and blocks in the part setting except needle point;
Step (2), at described silica-based or silicon carbide-based detecting probe surface by vacuum evaporation coating membrane technology evaporation or by the magnetron sputtering technique sputtering noble metal film of nano particle size, precious metal alloys film or noble metal lamination, and block described in removing;
Step (3), needle point strengthens and Raman spectrum TERS equipment applies obtained nano-probe carries out TERS experiment, and experimentally result adds up the corresponding relation of the enhanced propertied of described nano-probe and preparation technology parameter;
Step (4), adjusts described preparation technology parameter according to described corresponding relation, repeats step (1)-(4), until be met the nano-probe of default enhancing condition.
2. the method for claim 1, is characterized in that, arranges to block to comprise in the part except needle point: at the Wax-coated layer of described part except needle point, tygon organic coating or stickup barrier bed.
3. the method for claim 1, is characterized in that, described by vacuum evaporation coating membrane technology evaporation or by magnetron sputtering technique sputtering nano particle size precious metal alloys film comprise:
The gold and silver target that molar ratio is 1:1 to 1:3 is set, uses described gold and silver target that described precious metal alloys film is set.
4. the method for claim 1, is characterized in that, described by vacuum evaporation coating membrane technology evaporation or by magnetron sputtering technique sputtering nano particle size noble metal lamination comprise:
Two or more noble metal target material is set simultaneously, is used alternatingly described two or more noble metal target material and carries out evaporation or sputtering obtains noble metal lamination.
5. method as claimed in claim 4, is characterized in that, described two or more noble metal target material comprises gold and silver-colored target, carries out evaporation or sputtering obtains Yin-Jin-Yin lamination according to order that is silver-colored, gold, silver target.
6. the method as described in any one of claim 1-5, is characterized in that, also comprises before step (2):
Between described silica-based or silicon carbide-based probe and noble metal target material, precious metal network is set, the closer to needle point position described in the density of mesh of precious metal network less.
7. method as claimed in claim 6, it is characterized in that, described precious metal network comprises the structure with the proportional amplification of needle point of described silica-based or silicon carbide-based probe, and the needle point of described silica-based or silicon carbide-based probe is contained in described precious metal network.
8. the method as described in any one of claim 1-5, is characterized in that, also comprises: heat described silica-based or silicon carbide-based probe before step (2).
9. the method as described in any one of claim 1-5, is characterized in that, step (1) comprising: with an organic solvent wash described silica-based or silicon carbide-based detecting probe surface, or uses silica-based or silicon carbide-based detecting probe surface described in sand papering; Or use deionized water-absolute ethyl alcohol-acetone-absolute ethyl alcohol-deionized water to described silica-based or silicon carbide-based detecting probe surface ultrasonic cleaning five minutes respectively, then vacuum drying treatment is carried out to the described silica-based or silicon carbide-based probe after cleaning.
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| CN105403551B (en) * | 2015-10-30 | 2018-02-09 | 上海纳米技术及应用国家工程研究中心有限公司 | A kind of preparation method with Raman-enhancing energy film |
| CN107267940B (en) * | 2017-06-09 | 2019-06-18 | 中国科学院合肥物质科学研究院 | A kind of Au-Cu/Ag-Al nano-multilayer film surface-enhanced fluorescence substrate and its application |
| CN109487221B (en) * | 2018-12-12 | 2021-04-02 | 中国科学院合肥物质科学研究院 | Ag-Au-Al-Cr-Cu nano composite film surface enhanced fluorescent substrate and preparation method thereof |
| CN110373708B (en) * | 2019-07-31 | 2021-04-30 | 东南大学 | Nano needle tip preparation platform and method for adjusting concentration to realize needle tip cone angle control |
| CN112481582B (en) * | 2020-12-22 | 2024-04-05 | 珠海拓优电子有限公司 | Nano-coating probe and preparation method thereof |
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